CN106756043A - The separation method of chromium and iron in a kind of hydrochloric acid system - Google Patents
The separation method of chromium and iron in a kind of hydrochloric acid system Download PDFInfo
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- CN106756043A CN106756043A CN201611180944.7A CN201611180944A CN106756043A CN 106756043 A CN106756043 A CN 106756043A CN 201611180944 A CN201611180944 A CN 201611180944A CN 106756043 A CN106756043 A CN 106756043A
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- chromium
- iron
- hydrochloric acid
- extractant
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 106
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 50
- 239000011651 chromium Substances 0.000 title claims abstract description 43
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 40
- 238000000926 separation method Methods 0.000 title claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 41
- 238000000605 extraction Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 32
- 229910021555 Chromium Chloride Inorganic materials 0.000 claims abstract description 29
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003513 alkali Substances 0.000 claims abstract description 16
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 claims abstract description 16
- 238000001556 precipitation Methods 0.000 claims abstract description 15
- 229910000604 Ferrochrome Inorganic materials 0.000 claims abstract description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 14
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 14
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 13
- 235000014413 iron hydroxide Nutrition 0.000 claims abstract description 13
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 13
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims abstract description 13
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 13
- 150000003839 salts Chemical class 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 8
- 229960005191 ferric oxide Drugs 0.000 claims abstract description 8
- 238000002386 leaching Methods 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 239000012074 organic phase Substances 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 239000001062 red colorant Substances 0.000 claims abstract description 5
- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 claims description 11
- 239000012071 phase Substances 0.000 claims description 9
- 238000009713 electroplating Methods 0.000 claims description 6
- 239000010802 sludge Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 241001347978 Major minor Species 0.000 claims description 3
- 239000003085 diluting agent Substances 0.000 claims description 3
- 239000000839 emulsion Substances 0.000 claims description 3
- 239000003350 kerosene Substances 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229940062993 ferrous oxalate Drugs 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910000151 chromium(III) phosphate Inorganic materials 0.000 description 2
- IKZBVTPSNGOVRJ-UHFFFAOYSA-K chromium(iii) phosphate Chemical compound [Cr+3].[O-]P([O-])([O-])=O IKZBVTPSNGOVRJ-UHFFFAOYSA-K 0.000 description 2
- -1 iron ion Chemical class 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/02—Oxides or hydrates thereof
- C01G37/033—Chromium trioxide; Chromic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/04—Chromium halides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/10—Halides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses the separation method of chromium and iron in a kind of hydrochloric acid system.It is comprised the following steps that：1st, salt Ore Leaching carbon ferrochrome gained chromium chloride and frerrous chloride mixed solution, first with hydrogen peroxide Fe2+It is fully oxidized to Fe3+, then according to iron-holder in solution, according to suitably comparing, add extractant to be extracted, it is mutually chromium chloride solution that water is obtained after extraction, and the back extraction of organic phase water obtains ferric chloride solution and extractant, and extractant is recycled；2nd, chromium chloride solution obtains chromium chloride crystal using direct crystallization method, it would however also be possible to employ plus alkali neutralization precipitation method is obtained chromium hydroxide, chromium hydroxide obtains chrome green through high-temperature calcination again；3rd, ferric chloride solution can directly be used as water purification agent, it would however also be possible to employ plus alkali neutralization precipitation method is obtained iron hydroxide, iron hydroxide obtains ferric oxide red colorant through high-temperature calcination again.Present invention process is simple, it is easy to operate, except iron rate is up to more than 99.95%.
Description
Technical field
The present invention relates to molten production chromic salts and the electroplating sludge hydrochloric acid leachate processing technology field of ferrochrome acid, specifically relate to
And in a kind of hydrochloric acid system chromium and iron separation method.
Background technology
In molten production chromic salts and electroplating sludge hydrochloric acid leachate processing technology field, particularly the carbon ferrochrome hydrochloric acid of ferrochrome acid
During leaching production chromic salts, because chromium and ferro element chemical property are close, with absorption-co-precipitation effect so that separation is removed
Iron turns into problem, and the method that chromium, iron are separate in current existing hydrochloric acid medium mainly has：（1）The ferrous oxalate precipitation method, are to utilize
The low principle of ferrous oxalate solubility product, is precipitated by ferrous oxalate and reaches the purpose that chromium, iron are separate, but the method is except iron rate
98% or so can be reached, it is impossible to yield products of quality, and except iron rate is to factors such as oxalic acid addition, reaction temperature, solution pH values
Extremely sensitive, operating difficulties, hydrochloric acid medium is more difficult to implement than sulfuric acid medium.（2）Oxidation neutralization precipitation method, using oxygen such as hydrogen peroxide
Agent is the Fe in leachate2+It is oxidized to Fe3+, then add alkali to neutralize, by controlling PH=2~3, generation Fe (OH)3Precipitation, then
Through filtering, the purpose that chromium, iron are separate is reached.The method is extremely sensitive to factors such as reaction temperature, solution pH values except iron rate, pH value
Height is high except iron rate, but the loss of chromium is big, and pH value is low except iron rate is low, it is impossible to reach de-ferrous effect, and the Fe (OH) for producing3Colloid
It is allowed to filter extremely difficult, while adsorb chromium ion causing damage.（3）Phosphate removes iron processes, China Patent No.
201310008212X, discloses the chromium and iron selective separation method in a kind of hydrochloric acid system solution, with electroplating sludge containing ferrochrome
Hydrochloric acid leachate is raw material, first adds alkali adjustment solution pH value to be 2.0 or so, soluble phosphate is subsequently adding, in optimum response
Stirring reaction 2 hours under the conditions of 90 DEG C of temperature, generation chromium phosphate and chromium hydroxide complex precipitate, be separated by filtration chromium and
Iron.Although the method can realize the separation of chromium and iron, except iron rate can only achieve 98% or so, and chromium loss is big, and higher
Reaction temperature and the reaction time more long can cause the rising of cost surely, most obvious defect is that heavy chromium reaction is compared pH value
Sensitivity, slightly mistake will produce the complex precipitate of colloidal chromium phosphate and chromium hydroxide so that filtering is extremely difficult.（4）
Solvent extraction, have been reported that in hydrochloric acid medium using TBP extract chromium or P204 extraction iron method separate chromium and iron, but this two kinds
There is chromium and iron common extraction in extractant, separating effect is bad, and except iron rate is low, chromium loss is big.Also have been reported that and use lauryl amine
Or the method that octadecylamine carries out extract and separate chromium and iron as extractant, although the method can reach 99% except iron rate, require
There is chromium and iron common extraction in solution pH value, emulsion is serious in extraction process 2 or so, in order to solve emulsification problem, need
Temperature that will be higher（80 DEG C optimal）, while also need to add the demulsifiers such as sodium chloride, and the back extraction of iron ion is also more difficult, mesh
Preceding this method still rests on the laboratory research stage, cannot also realize industrialized production.
In sum, the present invention devises the separation method of chromium and iron in a kind of new hydrochloric acid system.
The content of the invention
For not enough present on prior art, the present invention seeks to be provide chromium and iron in a kind of hydrochloric acid system point
From method, process is simple, it is easy to operate, except iron rate is up to more than 99.95%.
To achieve these goals, the present invention is to realize by the following technical solutions：In a kind of hydrochloric acid system chromium and
The separation method of iron, it is comprised the following steps that：1st, salt Ore Leaching carbon ferrochrome gained chromium chloride and frerrous chloride mixing are molten
Liquid, first with hydrogen peroxide Fe2+It is fully oxidized to Fe3+, then according to iron-holder in solution, according to suitably comparing, add extraction
Agent is extracted, and it is mutually chromium chloride solution that water is obtained after extraction, and the back extraction of organic phase water obtains ferric chloride solution and extractant,
Extractant is recycled；2nd, chromium chloride solution obtains chromium chloride crystal using direct crystallization method, it would however also be possible to employ plus alkali is neutralized
Intermediate processing is obtained chromium hydroxide, and chromium hydroxide obtains chrome green through high-temperature calcination again；3rd, ferric chloride solution can be direct
It is used as water purification agent, it would however also be possible to employ plus alkali neutralization precipitation method is obtained iron hydroxide, iron hydroxide obtains oxygen through high-temperature calcination again
Change iron oxide red pigment.
Salt Ore Leaching carbon ferrochrome gained chromium chloride and frerrous chloride mixed solution in described step 1 can be replaced it
The hydrochloric acid leachate of its ferrochrome, can also be the electroplating sludge hydrochloric acid leachate containing chromium and iron.
Extractant in described step 1 uses sec-octyl alcohol or sec-octyl alcohol and N235Mixture, using sulfonated kerosene as
Diluent, preferably sec-octyl alcohol.
Extraction in described step 1 and back extraction can be carried out at normal temperatures, and it is short that two-phase reaches the extraction equilibrium time, no
Emulsion is produced, split-phase is fast.
Extractant in described step 1 is recycled, and gained major-minor product is free of Cr6+。
Beneficial effects of the present invention：Compared with the existing technical method from the acid mixed solution of chromium and iron except iron,
Advantage the most prominent is process is simple, it is easy to operated, except iron rate is up to more than 99.95%, chromium not common extraction, chromium free of losses, gained
Product high-quality, low cost, extractant are recycled, and without " three wastes " discharge, major-minor product is free of Cr6+, meet national chromium row
Industry cleaner production policy, is typical new cleanproduction process, for the sound development of Chrome Salt Industry provides a new approach.
Brief description of the drawings
Describe the present invention in detail with reference to the accompanying drawings and detailed description；
Fig. 1 is process chart of the invention.
Specific embodiment
For technological means, creation characteristic, reached purpose and effect for making present invention realization are easy to understand, with reference to
Specific embodiment, is expanded on further the present invention.
Reference picture 1, this specific embodiment uses following technical scheme：The separation side of chromium and iron in a kind of hydrochloric acid system
Method, it is comprised the following steps that：1st, salt Ore Leaching carbon ferrochrome gained chromium chloride and frerrous chloride mixed solution, first use dioxygen
Water is Fe2+It is fully oxidized to Fe3+, then according to iron-holder in solution, according to suitably comparing, add extractant to be extracted,
It is mutually chromium chloride solution that water is obtained after extraction, and the back extraction of organic phase water obtains ferric chloride solution and extractant, extractant circulation
Use；2nd, chromium chloride solution obtains chromium chloride crystal using direct crystallization method, it would however also be possible to employ plus alkali neutralization precipitation method system
Chromium hydroxide is obtained, chromium hydroxide obtains chrome green through high-temperature calcination again；3rd, ferric chloride solution can directly be used as water purification agent,
Can also be using adding alkali neutralization precipitation method that iron hydroxide is obtained, iron hydroxide obtains ferric oxide red colorant through high-temperature calcination again.
Embodiment 1：Chromium chloride and frerrous chloride mixed liquor obtained by salt Ore Leaching carbon ferrochrome as raw material, in solution
Cr3+Concentration is 120.6g/l, Fe2+Concentration is 56.5g/l, according to Fe2+Content adds appropriate hydrogen peroxide, and stirring makes Fe under normal temperature2+
It is fully oxidized to Fe3+, it is subsequently adding sec-octyl alcohol extractant and is extracted, extraction phase compares O/A=2：1, through three-level counter-current extraction, obtain
To water phase chromium chloride solution in Cr3+Concentration is 120.6g/l, Fe2+Concentration is 0.005g/l, except iron rate 99.99%, does not extract chromium,
Chromium chloride solution obtains chromium chloride crystal using direct crystallization method, it would however also be possible to employ plus alkali neutralization precipitation method is obtained hydroxide
Chromium, chromium hydroxide obtains chrome green through high-temperature calcination again；The back extraction of organic phase water obtains extractant sec-octyl alcohol and chlorination
O/A=0.5 is compared in ferrous solution, back extraction：1, the back extraction ratio 100% of iron, extractant is recycled, and ferric chloride solution can directly be used as
Water purification agent, it would however also be possible to employ plus alkali neutralization precipitation method is obtained iron hydroxide, iron hydroxide obtains iron oxide through high-temperature calcination again
Red.
Embodiment 2：It is raw material with the electroplating sludge hydrochloric acid leachate containing chromium and iron, Cr in solution3+Concentration is 18g/l, Fe2 +Concentration is 12g/l, according to Fe2+Content adds appropriate hydrogen peroxide, and stirring makes Fe under normal temperature2+It is completely converted into Fe3+, it is subsequently adding
Sec-octyl alcohol extractant is extracted, and extraction phase compares O/A=1：1, extracted through two stage countercurrents, Cr in the water phase chromium chloride solution for obtaining3+
Concentration is 18g/l, and Fe2+ concentration is 0.002g/l, except iron rate 99.98%, does not extract chromium, and chromium chloride solution uses direct crystallization method
Obtain chromium chloride crystal, it would however also be possible to employ plus alkali neutralization precipitation method is obtained chromium hydroxide, chromium hydroxide is obtained through high-temperature calcination again
To chrome green；The back extraction of organic phase water obtains extractant sec-octyl alcohol and ferric chloride solution, and O/A=1 is compared in back extraction：1, iron
Back extraction ratio 100%, extractant recycles, and ferric chloride solution can directly be used as water purification agent, it would however also be possible to employ plus in alkali and heavy
Shallow lake method is obtained iron hydroxide, and iron hydroxide obtains ferric oxide red colorant through high-temperature calcination again.
Embodiment 3：Chromium chloride and frerrous chloride mixed solution obtained by salt Ore Leaching carbon ferrochrome as raw material, in solution
Cr3+Concentration is 118g/l, Fe2+Concentration is 55.8g/l, according to Fe2+Content adds appropriate hydrogen peroxide, and stirring makes Fe under normal temperature2+Entirely
Portion changes into Fe3+, it is subsequently adding extractant and is extracted, extractant composition is N235 and the mixture of sec-octyl alcohol, sulfonated kerosene
It is diluent, extraction phase compares O/A=1：1, through three-level counter-current extraction, Cr in the water phase chromium chloride solution for obtaining3+Concentration is 118g/
L, Fe2+Concentration is 0.02g/l, except iron rate 99.96%, does not extract chromium, and it is brilliant that chromium chloride solution obtains chromium chloride using direct crystallization method
Body, it would however also be possible to employ plus alkali neutralization precipitation method is obtained chromium hydroxide, chromium hydroxide obtains chrome green through high-temperature calcination again；
The back extraction of organic phase water obtains extractant sec-octyl alcohol and ferric chloride solution, and O/A=1 is compared in back extraction：1, the back extraction ratio 100% of iron,
Extractant is recycled, and ferric chloride solution can directly be used as water purification agent, it would however also be possible to employ plus alkali neutralization precipitation method is obtained hydrogen
Iron oxide, iron hydroxide obtains ferric oxide red colorant through high-temperature calcination again.
General principle of the invention and principal character and advantages of the present invention has been shown and described above.The technology of the industry
Personnel it should be appreciated that the present invention is not limited to the above embodiments, simply explanation described in above-described embodiment and specification this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appending claims and its
Equivalent thereof.
Claims (6)
1. in a kind of hydrochloric acid system chromium and iron separation method, it is characterised in that it is comprised the following steps that：(1), salt acidleach
Go out carbon ferrochrome gained chromium chloride and frerrous chloride mixed solution, first with hydrogen peroxide Fe2+It is fully oxidized to Fe3+, then basis
Iron-holder in solution, adds extractant to be extracted, and it is mutually chromium chloride solution that water is obtained after extraction, and organic phase water is stripped
To ferric chloride solution and extractant, extractant recycling；(2), chromium chloride solution obtains chromium chloride using direct crystallization method
Crystal, or using adding alkali neutralization precipitation method that chromium hydroxide is obtained, chromium hydroxide obtains chrome green through high-temperature calcination again；
(3), ferric chloride solution is directly used as water purification agent, or using adding alkali neutralization precipitation method that iron hydroxide is obtained, iron hydroxide is passed through again
High-temperature calcination obtains ferric oxide red colorant.
2. in a kind of hydrochloric acid system according to claim 1 chromium and iron separation method, it is characterised in that described step
(1) salt Ore Leaching carbon ferrochrome gained chromium chloride and frerrous chloride mixed solution in replace with the hydrochloric acid leachate of ferrochrome
Or the electroplating sludge hydrochloric acid leachate containing chromium and iron.
3. in a kind of hydrochloric acid system according to claim 1 chromium and iron separation method, it is characterised in that described step
(1) extractant in uses sec-octyl alcohol and N235Mixture, using sulfonated kerosene as diluent.
4. in a kind of hydrochloric acid system according to claim 1 chromium and iron separation method, it is characterised in that described step
(1) extractant in uses sec-octyl alcohol.
5. in a kind of hydrochloric acid system according to claim 1 chromium and iron separation method, it is characterised in that described step
(1) extraction in and back extraction can be carried out at normal temperatures, and it is short that two-phase reaches the extraction equilibrium time, does not produce emulsion, point
It is mutually fast.
6. in a kind of hydrochloric acid system according to claim 1 chromium and iron separation method, it is characterised in that described step
(1) extractant in is recycled, and gained major-minor product is free of Cr6+。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611180944.7A CN106756043A (en) | 2016-12-20 | 2016-12-20 | The separation method of chromium and iron in a kind of hydrochloric acid system |
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| CN201611180944.7A CN106756043A (en) | 2016-12-20 | 2016-12-20 | The separation method of chromium and iron in a kind of hydrochloric acid system |
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| CN201611180944.7A Pending CN106756043A (en) | 2016-12-20 | 2016-12-20 | The separation method of chromium and iron in a kind of hydrochloric acid system |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109536708A (en) * | 2018-12-17 | 2019-03-29 | 江苏永葆环保科技有限公司 | The separation method of chromium and iron in a kind of pickle liquor |
| CN110724837A (en) * | 2019-10-23 | 2020-01-24 | 金川集团股份有限公司 | Method for selectively separating iron and chromium in hydrochloric acid system solution |
| CN112661196A (en) * | 2020-12-29 | 2021-04-16 | 斯瑞尔环境科技股份有限公司 | Purification method of ferric trichloride |
| CN118099495A (en) * | 2023-09-28 | 2024-05-28 | 斯瑞尔环境科技股份有限公司 | Method for preparing iron-chromium electrolyte by leaching carbon ferrochromium with ferric trichloride |
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| RU2052520C1 (en) * | 1993-01-11 | 1996-01-20 | Салимжан Хаирович Кусембаев | Method for reprocessing disintegrating metallurgical slags |
| CN102660678A (en) * | 2012-05-17 | 2012-09-12 | 四川大学 | Method for selectively separating iron from hydrochloric acid solution containing ferrous chloride |
| CN105018732A (en) * | 2015-07-01 | 2015-11-04 | 夏栋 | Novel method for comprehensive recovery of etching waste liquid and waste residues |
| CN105543506A (en) * | 2016-02-19 | 2016-05-04 | 马桂文 | Method for producing high-purity chromium metal |
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| RU2052520C1 (en) * | 1993-01-11 | 1996-01-20 | Салимжан Хаирович Кусембаев | Method for reprocessing disintegrating metallurgical slags |
| CN102660678A (en) * | 2012-05-17 | 2012-09-12 | 四川大学 | Method for selectively separating iron from hydrochloric acid solution containing ferrous chloride |
| CN105018732A (en) * | 2015-07-01 | 2015-11-04 | 夏栋 | Novel method for comprehensive recovery of etching waste liquid and waste residues |
| CN105543506A (en) * | 2016-02-19 | 2016-05-04 | 马桂文 | Method for producing high-purity chromium metal |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109536708A (en) * | 2018-12-17 | 2019-03-29 | 江苏永葆环保科技有限公司 | The separation method of chromium and iron in a kind of pickle liquor |
| CN110724837A (en) * | 2019-10-23 | 2020-01-24 | 金川集团股份有限公司 | Method for selectively separating iron and chromium in hydrochloric acid system solution |
| CN112661196A (en) * | 2020-12-29 | 2021-04-16 | 斯瑞尔环境科技股份有限公司 | Purification method of ferric trichloride |
| CN118099495A (en) * | 2023-09-28 | 2024-05-28 | 斯瑞尔环境科技股份有限公司 | Method for preparing iron-chromium electrolyte by leaching carbon ferrochromium with ferric trichloride |
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